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    高效液相色谱法同时测定婴儿湿巾中9种防腐剂

    etermination of 9 Preservatives in Baby Wet Wipes by High Performance Liquid Chromatography

    • 摘要: 称取0.500 0 g湿巾样品,剪碎后,加入80%(体积分数)甲醇溶液5.00 mL,漩涡振荡提取3 min,经0.22 μm滤膜过滤,以Diamonsil C18(2)色谱柱(4.6 mm×250 mm,5 μm)分离滤液中的9种防腐剂,流动相为甲醇-0.1%(质量分数)磷酸溶液,梯度洗脱。采用二极管阵列检测器,咪唑烷基脲、5,5-二甲基海因、2-溴-2-硝基丙烷-1,3-二醇、苄索氯胺和苯扎氯铵的检测波长为210 nm,氯苯酣醚的检测波长为230 nm,醋酸氯己定、山梨酸钾和氯化十六烷基吡啶的检测波长为254 nm。9种防腐剂的质量浓度在一定范围内与对应的色谱峰面积呈线性关系,检出限(3S/N)在0.01~0.5 mg·L-1之间。对空白样品进行加标回收试验,回收率在77.2%~100%之间,测定值的相对标准偏差(n=6)在1.2%~8.4%之间。应用该方法分析了20批次婴儿湿巾样品,有15批次的样品中检出咪唑烷基脲、5,5-二甲基海因、2-溴-2-硝基丙烷-1,3-二醇、醋酸氯己定、山梨酸钾或苄索氯胺。

       

      Abstract: The wipe sample (0.500 0 g) was cut and extracted with 5.00 mL of 80% (volume fraction) methanol solution by vortex oscillation for 3 min. After filtrating through 0.22 μm filter membrane, 9 preservatives in the filtrate were separated on a Diamonsil C18 (2) column (4.6 mm×250 mm, 5 μm), with a mixture of methanol and 0.1% (mass fraction) phosphoric acid solution as mobile phase for gradient elution, and detected by a diode array detector, at the wavelength of 210 nm for imidazolidinyl urea, 5,5-dimethylhydantoin, 2-bromo-2-nitropropane-1,3-diol, benzethonamide and benzalkonium chloride, 230 nm for chlorobenzoate, 254 nm for chlorhexidine acetate, potassium sorbate and cetylpyridinium chloride. Linear relationships were found between chromatographic area peak and mass concentration of 9 preservatives in definite ranges, with detection limits (3S/N) in the range of 0.01-0.5 mg·L-1. Test for recovery was made by standard addition method on the base of blank sample, giving results in the range of 77.2%-100%, with the relative standard deviations (RSDs,n=6) ranged from 1.2% to 8.4%. The proposed method was used to analyze 20 batches of baby wet wipes, and imidazolidinyl urea, 5,5-dimethylhydantoin, 2-bromo-2-nitropropane-1,3-diol, chlorhexidine acetate, potassium sorbate, benzethonamide were found in 15 batches of samples.

       

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